Superplasticity and superionic conductivity (SIC), both thermally activated processes, have been independently observed in certain materials with a high diffusion coefficient in high temperature ranges. Intuitively, this observation leads one to the idea that both types of behavior may be inter-related with one another. Therefore, it is the purpose of this research to investigate, specifically, the deformation characteristics of two SIC's, Bi₂O₃ and YSZ (yttria-stabilized zirconia), and to attempt a correlation of their behavior. Compressive deformation of these two materials was conducted over a wide range of temperatures and at various strain rates in an effort to characterize the temperature and/or strain-rate dependences of any observed superplasticity. Steady-state flow stress values were utilized to calculate the strain-rate sensitivity, m, of the materials, as well as the activation energies (Q_C) of superplasticity. Next, the obtained values of Q_C. were compared to SIC activation energies from the literature. Bi₂O₃ exhibited structural superplasticity within the range of test conditions utilized. However, published values of SIC activation energy were lower than experimentally derived Q_C by a factor of four. Therefore, one is not able to state whether or not there is any correlation between the two behaviors. Unfortunately, YSZ exhibited brittle behavior over the entire temperature and strain-rate ranges, so the same analysis could not be performed. Furthermore, SEM micrographs showed that YSZ samples, as processed, did not possess the proper microstructure required for superplasticity. Hence, no final conclusions on YSZ can be drawn from this study. / Master of Science

This thesis was developed in the frame of a Brazil-France cooperation agreement between the École des Mines d\'Albi-Carmaux and the Polytechnic School of Engineering of the University of Sao Paulo (EPUSP). It aims to contribute to the study of the mechanical behaviour of Ti6Al4V alloys especially in terms of superplastic forming. The general objective of this research is to develop non-conventional forming processes for new titanium alloys applied to aerospace components Therefore, in accordance of the equipment\'s available in the two groups, the work will be conducted either at the Ecole des Mines d\'Albi-Carmaux and either at EPUSP. This thesis aims to answer questions such as what are the implications in relation to the microstructural and mechanical behaviour of these alloys during superplastic and hot forming in order to establish a behaviour law for these alloys based on titanium. This requires a good knowledge of the properties of materials used in the superplastic and hot forming domain to control the parameters governing the phenomenon of superplasticity or high temperature plasticity. For this, a testing strategy and characterization methodology of those new titanium alloys was developed. The tests include high temperature uniaxial tensile tests on several Ti6Al4V alloys showing different initial grain sizes. Special focus was made on the microstructural evolution prior to testing (i.e. during specimen temperature increase and stabilization) and during testing. Testing range was chosen to cover the hot forming and superplastic deformation domain. Grain growth is depending on alloy initial microstructures but also on the duration of the test at testing temperature (static growth) and testing strain rate (dynamic growth). After testing microstructural evolutions of the alloys will be observed by optical micrograph or SEM and results are used to increase behaviour model accuracy. Advanced unified behaviour models where introduced in order to cover the whole strain rate and temperature range: kinematic hardening, strain rate sensitive and grain growth features are included in the model. In order to get validation of the behaviour model, it was introduced in ABAQUSR numerical simulation code and model predictions (especially macroscopic deformation and local grain growth) were compared, for one of the material investigated, to axisymmetric inflation forming tests of sheet metal parts, also known as bulge test. To obtain a simple control cycle, tests performed at IPT/LEL laboratory in San José Dos Campos in Brazil were operated with a constant strain rate. Results show a very good correlation with predictions and allows to conclude on an accuracy of the behaviour models of the titanium alloys in industrial forming conditions. / Esta tese desenvolvida dentro do acordo de cooperação internacional celebrado entre a Escola Politécnica da Universidade de São Paulo (EPUSP) e a École des Mines d\'Albi-Carmaux tem como tema principal a análise da influência da evolução microestrutural sobre o comportamento mecânico de chapa de liga de titânio - Ti-6Al- 4V sob condições superplásticas e trabalho a quente. O objetivo desta pesquisa é contribuir para o desenvolvimento de processos de conformação não convencional de chapas de ligas a base de titânio utilizadas na manufatura de componentes metálicos. Como objetivo específico, estabelecer uma correlação entre comportamento mecânico e a mudança microestrutural a partir de três tipos de ligas com diferentes tamanhos de grão iniciais (0.5, 3.0 e 4.9 ?m). Os testes foram realizados na faixa de temperatura de 700 a 950 °C combinados às taxas de deformação na faixa de 10-1 s-1 - 10-4 s-1. Para a metodologia, estabeleceu-se uma estratégia de ensaios mecânicos capaz de testar as hipóteses sobre o comportamento do material formuladas no início desta pesquisa. Em seguida, os ensaios mecânicos foram divididos em três partes. Na primeira, utilizou-se um simulador termomecânico modelo Gleeble 3800 para os ensaios a quente variando-se a taxa de deformação (??) entre 10-1 s-1 a 10-3 s-1 e temperaturas da ordem de 700 °C a 850 °C. Na segunda parte dos testes, priorizouse taxas de deformação mais lentas (10-2 s-1 - 10-4 s-1) e temperaturas mais elevadas (800 °C - 950 °C) objetivando atingir as deformações superplásticas do material, nesta etapa utilizou-se como equipamento uma máquina de tração modelo MTS 50kN com câmara de aquecimento acoplada. A terceira parte dos ensaios experimentais envolveu a conformação na condição superplástica por pressão hidrostática (Bulge test) realizadas no LEL-IPT de São José dos Campos. A partir da análise dos dados experimentais levantou-se os parâmetros introduzidos no modelo numérico de comportamento mecânico baseado na evolução da microestrutura da chapa testada permitindo a calibração do modelo numérico a partir das equações constituintes e finalmente introduzido no software de elementos finitos (ABAQUS 6.12) e construído a simulação numérica da conformação superplástica por pressão hidrostática. Os principais resultados indicaram uma forte correlação entre microestrutura inicial da conformação superplástica e a quente de onde se pode observar que tanto menor a microestrutura inicial maior será a quantidade do crescimento de grão. Os resultados da conformação superplástica de expansão multiaxial do domo hemisférico foram, então, comparados à simulação numérica permitindo confrontar os dados do modelo numérico do comportamento mecânico com a lei de comportamento estudada, o que possibilitou um melhor entendimento dos mecanismos da conformação plástica em condições de superplasticidade e também de trabalho a aquente do material.

This thesis describes the effect of dislocation slip on superplastic deformation of AZ31 magnesium alloy. Through two different routes of ECAE (equal channel angular extrusion), two types of specimens having the same grain size but different texture were obtained. One is favorable for basal slip and the other is not. Under the same condition of deformation, the strain rate sensitivity and contribution of grain boundary sliding to total elongation in these two different specimens are almost the same. As for elongation, not much difference was found. The present results demonstrate that the relationship between dislocation slip and grain boundary sliding in superplastic AZ31 magnesium alloy is non-obvious.

This thesis was developed in the frame of a Brazil-France cooperation agreement between the École des Mines d\'Albi-Carmaux and the Polytechnic School of Engineering of the University of Sao Paulo (EPUSP). It aims to contribute to the study of the mechanical behaviour of Ti6Al4V alloys especially in terms of superplastic forming. The general objective of this research is to develop non-conventional forming processes for new titanium alloys applied to aerospace components Therefore, in accordance of the equipment\'s available in the two groups, the work will be conducted either at the Ecole des Mines d\'Albi-Carmaux and either at EPUSP. This thesis aims to answer questions such as what are the implications in relation to the microstructural and mechanical behaviour of these alloys during superplastic and hot forming in order to establish a behaviour law for these alloys based on titanium. This requires a good knowledge of the properties of materials used in the superplastic and hot forming domain to control the parameters governing the phenomenon of superplasticity or high temperature plasticity. For this, a testing strategy and characterization methodology of those new titanium alloys was developed. The tests include high temperature uniaxial tensile tests on several Ti6Al4V alloys showing different initial grain sizes. Special focus was made on the microstructural evolution prior to testing (i.e. during specimen temperature increase and stabilization) and during testing. Testing range was chosen to cover the hot forming and superplastic deformation domain. Grain growth is depending on alloy initial microstructures but also on the duration of the test at testing temperature (static growth) and testing strain rate (dynamic growth). After testing microstructural evolutions of the alloys will be observed by optical micrograph or SEM and results are used to increase behaviour model accuracy. Advanced unified behaviour models where introduced in order to cover the whole strain rate and temperature range: kinematic hardening, strain rate sensitive and grain growth features are included in the model. In order to get validation of the behaviour model, it was introduced in ABAQUSR numerical simulation code and model predictions (especially macroscopic deformation and local grain growth) were compared, for one of the material investigated, to axisymmetric inflation forming tests of sheet metal parts, also known as bulge test. To obtain a simple control cycle, tests performed at IPT/LEL laboratory in San José Dos Campos in Brazil were operated with a constant strain rate. Results show a very good correlation with predictions and allows to conclude on an accuracy of the behaviour models of the titanium alloys in industrial forming conditions. / Esta tese desenvolvida dentro do acordo de cooperação internacional celebrado entre a Escola Politécnica da Universidade de São Paulo (EPUSP) e a École des Mines d\'Albi-Carmaux tem como tema principal a análise da influência da evolução microestrutural sobre o comportamento mecânico de chapa de liga de titânio - Ti-6Al- 4V sob condições superplásticas e trabalho a quente. O objetivo desta pesquisa é contribuir para o desenvolvimento de processos de conformação não convencional de chapas de ligas a base de titânio utilizadas na manufatura de componentes metálicos. Como objetivo específico, estabelecer uma correlação entre comportamento mecânico e a mudança microestrutural a partir de três tipos de ligas com diferentes tamanhos de grão iniciais (0.5, 3.0 e 4.9 ?m). Os testes foram realizados na faixa de temperatura de 700 a 950 °C combinados às taxas de deformação na faixa de 10-1 s-1 - 10-4 s-1. Para a metodologia, estabeleceu-se uma estratégia de ensaios mecânicos capaz de testar as hipóteses sobre o comportamento do material formuladas no início desta pesquisa. Em seguida, os ensaios mecânicos foram divididos em três partes. Na primeira, utilizou-se um simulador termomecânico modelo Gleeble 3800 para os ensaios a quente variando-se a taxa de deformação (??) entre 10-1 s-1 a 10-3 s-1 e temperaturas da ordem de 700 °C a 850 °C. Na segunda parte dos testes, priorizouse taxas de deformação mais lentas (10-2 s-1 - 10-4 s-1) e temperaturas mais elevadas (800 °C - 950 °C) objetivando atingir as deformações superplásticas do material, nesta etapa utilizou-se como equipamento uma máquina de tração modelo MTS 50kN com câmara de aquecimento acoplada. A terceira parte dos ensaios experimentais envolveu a conformação na condição superplástica por pressão hidrostática (Bulge test) realizadas no LEL-IPT de São José dos Campos. A partir da análise dos dados experimentais levantou-se os parâmetros introduzidos no modelo numérico de comportamento mecânico baseado na evolução da microestrutura da chapa testada permitindo a calibração do modelo numérico a partir das equações constituintes e finalmente introduzido no software de elementos finitos (ABAQUS 6.12) e construído a simulação numérica da conformação superplástica por pressão hidrostática. Os principais resultados indicaram uma forte correlação entre microestrutura inicial da conformação superplástica e a quente de onde se pode observar que tanto menor a microestrutura inicial maior será a quantidade do crescimento de grão. Os resultados da conformação superplástica de expansão multiaxial do domo hemisférico foram, então, comparados à simulação numérica permitindo confrontar os dados do modelo numérico do comportamento mecânico com a lei de comportamento estudada, o que possibilitou um melhor entendimento dos mecanismos da conformação plástica em condições de superplasticidade e também de trabalho a aquente do material.

Le formage superplastique (SuperPlastic Forming, SPF) permet d'élaborer des pièces de forme complexe qui, de par les matériaux employés, allient faible densité et haute résistance mécanique. Toutefois, sa mise en œuvre nécessite la connaissance de la loi de pression à appliquer afin de contrôler l'endommagement tout comme la répartition d'épaisseur au sein de la pièce. Il est ainsi nécessaire de mettre en place des simulations numériques pour déterminer les conditions optimales du formage. L'exactitude des prédictions obtenues repose alors sur la description du comportement et de l'endommagement du matériau soumis à des conditions thermomécaniques représentatives du procédé considéré. Le présent travail propose donc une modélisation du comportement et de l'endommagement de l'alliage d'aluminium 7475 via une étude comparative de divers modèles. Les travaux peuvent ainsi être divisés en trois grandes étapes : (i) la caractérisation du comportement de l'alliage ; (ii) la caractérisation de l'endommagement de l'alliage et (iii) la mise en place de simulations numériques pour des formes types. Des essais de traction uniaxiale à chaud ont été réalisés afin de caractériser le comportement de l'alliage 7475. Une modélisation de ce-dernier par trois modèles (Norton-Hoff, Johnson-Cook et Zener-Hollomon) est proposée. Les résultats obtenus montrent que le modèle de Zener-Hollomon conduit à la meilleure description du comportement rhéologique de l'alliage dans les conditions thermomécaniques étudiées. Par la suite, l'endommagement de l'alliage 7475 dans des conditions représentatives du formage superplastique a été étudié. Un critère de type Gurson est proposé. Des observations par micro-tomographie aux rayons X ont d'ailleurs permis d'étudier plus précisément l'évolution de l'endommagement au cours de la déformation. À partir de ces résultats, des simulations numériques par éléments finis (sous ABAQUS) ont été mises en place. / Superplasticity is the ability of some materials to sustain very high value of strain (up to 2000%) under low stress and within a specific range of temperature and strain rate. Complex shape components combining low density and high strength can thus be elaborated by using this peculiar characteristic. Superplastic forming process consists in deforming a flange by applying a variable pressure until the flange takes the form of a die. A good knowledge of the pressure law to apply is therefore primordial in order to avoid damage and obtain homogeneous thickness distribution. Numerical simulations are generally used to predict the optimal forming conditions. But a precise description of the rheological response of the material (in terms of flow rule and damage evolution) under thermomechanical conditions representative of the process is necessary. The PhD work introduces several rheological models to describe the behavior of a 7xxx aluminum alloy during superplastic forming process. The work is divided into three parts: (i) characterization of rheological models, (ii) characterization of damage models and (iii) development of numerical simulations to predict the superplastic forming of typical shapes. Hot uniaxial tensile tests have been performed to characterize the rheological behavior of a 7475 alloy. Three models (i.e. Norton-Hoff, Johnson-Cook and Zener-Hollomon) have been identified but only the last one leads to a good prediction of the material response. A GTN damage model has also been identified. Observations by X-rays micro-tomography have allowed studying in more details the damage evolution during the deformation. From these results, different cases have been simulated in ABAQUS.

Esta tese tem por objetivo determinar a estampabilidade de chapas de alumínio 5083 O processadas pelo processo de fricção e mistura (PFM). Para atingir os objetivos propostos o processo de fricção por mistura foi estudado e uma ferramenta de soldagem PFM construída, a verificação da qualidade da solda foi realizada com metalografia da região processada para verificar a presença de vazios, obtidas as melhores condições a superplasticidade através do processo PFM é estudada com os ensaios de tração a quente e de saltos. Ensaios de tração a frio foram realizados nos corpos de prova com o processamento e sem o processamento com o objetivo de obter a curva tensão versus deformação do material processado e sem processamento. Foi efetuado o ensaio de microdureza da região soldada. A estampabilidade das chapas foi verificada através do ensaio de expansão hidrostática e empregadas na determinação da conformabilidade das chapas processadas e sem processar. Os ensaios de expansão hidrostática foram realizados em software de elementos finitos com o objetivo de comparar os resultados práticos e teóricos. Este estudo simulou pelo método dos elementos finitos a determinação da curva limite de conformação de chapas de alumínio 5083 O processadas através do processo PFM. A simulação de elementos finitos implicou em utilizar o método não linear e os softwares MSC MARC e Abaqus para simulação. Determinou-se neste estudo que a resistência à tração de chapas após processo PFM é 30% maior do que sem processamento, a estampabilidade à frio das chapas manteve-se a mesma. Os testes práticos determinaram que os softwares Abaqus e MSC MARC possuem boa aproximação para o teste de expansão hidrostática à frio. O Software Abaqus apresentou dificuldades para convergir e tempo de processamento muito superior ao MSC MARC nos estudos de expansão hidrostática à frio e na condição superplástica. Através dos ensaios de saltos determinou-se que a condição 328 rpm e 65 mm/min possui coeficiente de sensibilidade à taxa de deformação m muito superior ao do alumínio 5083 O sem PFM, isto resultou em uma melhor distribuição de espessura da chapa após o ensaio de expansão hidrostática superplástico em software. / The aim of this study is to determine the sheet metal formability of 5083 O aluminum sheets after friction stir processing \"FSP\". To achieve the proposed objectives the friction stir processing was be reviewed and modeled in order to enable the design and manufacture of a proper FSP tool. The quality of the process was carried out through metallographic tests of the FSP region looking for the presence of voids. The best conditions for plasticity and superplastic forming after FSP was studied by means of an approach of jump steps in the hot tensile tests, looking for a coefficient of strain rate sensitivity. The micro hardness tests and tensile tests at room temperature were carried out for the specimens with and without FSP processing in order to characterize their material mechanical behavior. The formability of the FSP blanks was evaluated through Bulge tests. The results enable to plot Forming Limit Curves friction stir processed blanks after FSP and without FSP. The numerical simulation of the Free Bulge tests was carried out using a Finite Element Method model in order to compare the numerical theoretical and experimental practical results. The numerical simulation approach allows for the determination the forming limit curve of 5083 O aluminum sheets processed by the FSP process. The Finite Element Method modeling and simulation have employed two nonlinear FEM codes: the MSC MARC and Abaqus were compared as software for the simulations. The Yeld Strength of specimens with FSP increased 30% in comparison with specimens without FSP in cold tensile tests, the formability of shapes with and without FSP was de same. The practical tests showed that Abaqus and MSC MARC results has a good approach, the processing time in Abaqus was much greater than in MSC MARC, Abaqus had convergence problems when contact condition is applied. Through the jump tensile tests the 328 rpm and 65 mm/min condition showed a m factor much higher in comparison with condition without FSP in AA 5083 O, this results led in a better thickness distribution after the superplastic bulge test in software.

L’objectif de cette étude est de quantifier la contribution intra et intergranulaire lors d’une sollicitation à haute température d’un alliage de magnésium (AZ31). Afin de répondre à cette problématique scientifique, un essai de traction in situ à haute température dans un MEB a été mis en place. Un important travail de développement a été réalisé autour de cet essai afin de lever un nombre de verrous technique conséquent. Ces verrous expliquent en partie pourquoi il existe aujourd’hui peu d’étude in situ à haute température sur des alliages de magnésium. Un marqueur local ayant la forme d’une microgrille a été déposé sur notre échantillon étant donné que celui-ci n’offre aucun contraste local pour la corrélation d’image numérique (CIN). Afin le dépôt du marqueur local, une cartographie EBSD a été réalisée. À l’aide des joints de grains issus de la carte EBSD, on peut venir superposer les joints de grains aux champs de déformation issue de la CIN.À l’aide des essais de traction in situ à haute température, on a pu mettre en avant l’effet de la température sur les différents mécanismes de déformation actif. Tout ce travail de développement nous permet ainsi de pouvoir localiser les hétérogénéités de déformation plastique à la fois en fonction de l’évolution de la déformation et pour plusieurs températures. D’après les essais menés, on a pu mettre en évidence le fait que plus la température est élevée, que plus les hétérogénéités de déformation plastique se localisent au voisinage des joints de grains. Basé sur une hypothèse cœur/manteau, on a pu venir quantifier la contribution intergranulaire, et mettre en avant que celle-ci devenait plus importante avec la température. / The aim of this study is to quantify the intra and intergranular contribution of the deformation during a high temperature micromechanical test on a magnesium alloy (AZ31). In order to answer this scientific issue, we have developed an in situ tensile test at high temperature within a SEM. It has required a significant preparation work in order to push the current technical limits of this type of test on magnesium alloy. These technical limits can partly explain why there are currently few in situ studies at high temperature on magnesium alloys. A local marker in the form of a microgrid was placed on our sample as it does not provide any local contrast for digital image correlation (DIC). Before the deposition of the microgrid, EBSD mapping was made. Using the grain boundaries from the EBSD, we can superimpose the deformed grain boundaries on the strain map from the DIC.Using high temperature in-situ tensile tests, we were able to highlight the effect of the temperature on the different active deformation mechanisms. This whole development work enables us to locate the plastic deformation heterogeneities both according to the evolution of the deformation and for several temperatures. From the tests conducted, it has been shown that the higher the temperature, the more heterogeneous the plastic deformation heterogeneities are located in the vicinity of the grain boundaries. Based on a heart/coat hypothesis, we were able to quantify the intra and intergranular contribution, and show that it became more important with temperature.

Esta tese tem por objetivo determinar a estampabilidade de chapas de alumínio 5083 O processadas pelo processo de fricção e mistura (PFM). Para atingir os objetivos propostos o processo de fricção por mistura foi estudado e uma ferramenta de soldagem PFM construída, a verificação da qualidade da solda foi realizada com metalografia da região processada para verificar a presença de vazios, obtidas as melhores condições a superplasticidade através do processo PFM é estudada com os ensaios de tração a quente e de saltos. Ensaios de tração a frio foram realizados nos corpos de prova com o processamento e sem o processamento com o objetivo de obter a curva tensão versus deformação do material processado e sem processamento. Foi efetuado o ensaio de microdureza da região soldada. A estampabilidade das chapas foi verificada através do ensaio de expansão hidrostática e empregadas na determinação da conformabilidade das chapas processadas e sem processar. Os ensaios de expansão hidrostática foram realizados em software de elementos finitos com o objetivo de comparar os resultados práticos e teóricos. Este estudo simulou pelo método dos elementos finitos a determinação da curva limite de conformação de chapas de alumínio 5083 O processadas através do processo PFM. A simulação de elementos finitos implicou em utilizar o método não linear e os softwares MSC MARC e Abaqus para simulação. Determinou-se neste estudo que a resistência à tração de chapas após processo PFM é 30% maior do que sem processamento, a estampabilidade à frio das chapas manteve-se a mesma. Os testes práticos determinaram que os softwares Abaqus e MSC MARC possuem boa aproximação para o teste de expansão hidrostática à frio. O Software Abaqus apresentou dificuldades para convergir e tempo de processamento muito superior ao MSC MARC nos estudos de expansão hidrostática à frio e na condição superplástica. Através dos ensaios de saltos determinou-se que a condição 328 rpm e 65 mm/min possui coeficiente de sensibilidade à taxa de deformação m muito superior ao do alumínio 5083 O sem PFM, isto resultou em uma melhor distribuição de espessura da chapa após o ensaio de expansão hidrostática superplástico em software. / The aim of this study is to determine the sheet metal formability of 5083 O aluminum sheets after friction stir processing \"FSP\". To achieve the proposed objectives the friction stir processing was be reviewed and modeled in order to enable the design and manufacture of a proper FSP tool. The quality of the process was carried out through metallographic tests of the FSP region looking for the presence of voids. The best conditions for plasticity and superplastic forming after FSP was studied by means of an approach of jump steps in the hot tensile tests, looking for a coefficient of strain rate sensitivity. The micro hardness tests and tensile tests at room temperature were carried out for the specimens with and without FSP processing in order to characterize their material mechanical behavior. The formability of the FSP blanks was evaluated through Bulge tests. The results enable to plot Forming Limit Curves friction stir processed blanks after FSP and without FSP. The numerical simulation of the Free Bulge tests was carried out using a Finite Element Method model in order to compare the numerical theoretical and experimental practical results. The numerical simulation approach allows for the determination the forming limit curve of 5083 O aluminum sheets processed by the FSP process. The Finite Element Method modeling and simulation have employed two nonlinear FEM codes: the MSC MARC and Abaqus were compared as software for the simulations. The Yeld Strength of specimens with FSP increased 30% in comparison with specimens without FSP in cold tensile tests, the formability of shapes with and without FSP was de same. The practical tests showed that Abaqus and MSC MARC results has a good approach, the processing time in Abaqus was much greater than in MSC MARC, Abaqus had convergence problems when contact condition is applied. Through the jump tensile tests the 328 rpm and 65 mm/min condition showed a m factor much higher in comparison with condition without FSP in AA 5083 O, this results led in a better thickness distribution after the superplastic bulge test in software.

Superplastic deformation behaviour of AZ31 magnesium alloy having initial grain sizes 8, 11 and 17μm alloy was investigated at 673 K with initial strain rates ranging from 1x10-2 to 1x10-4 s-1. Mechanical data on fine grained AZ31 alloy with grain sizes 8 and 11 μm indicated a transition in deformation mechanisms. The strain rate sensitivity, m ~ 0.5 at low strain rates and m ~ 0.2 at high strain rates which suggest GBS and dislocation slip as the corresponding deformation mechanism. For coarse grained alloy having grain size 17 μm, m < 0.4 at low strain rates and ~ 0.2 at high strain rates, suggesting dislocation slip as the deformation mechanism. A superplastic maximum elongation of ~ 475% was observed for 8 μm alloy at low rate of deformation. At high strain rates, the deformation was non-superplastic for fine and coarse grained alloys. The contribution of GBS to total strain, ξ in the low strain rate regime was evaluated to be 50 – 60%, for both low and high elongation. EBSD studies indicated the maintenance of high fraction of high angle boundaries up to true strain of ~ 0.88 and a reduction in texture intensity. These observations show GBS as the dominant deformation mechanism for fine grained alloy. At higher strain rate, ξ was estimated to be 30%. Fraction of high angle boundaries was reduced and [0001] direction of grains was found to be rotated towards the tensile direction, suggesting dislocation slip. Based on mechanical data, flow localization and cavitation studies; the failure of the material during high rates of deformation was mainly due to flow localization. Extensive cavitation along with more uniform flow at a lower strain rate regime suggests the failure due to the cavity interlinkage and coalescence. The present GBS data are consistent with the previous relevant data in fine grained Mg based alloys in the low strain rate regime. The GBS data obtained in the dislocation regime in the present study are also in agreement with that of the previous investigations in fine grained Mg alloys.

Dans le cadre du programme de recherche sur les matériaux de gainage pour les réacteurs à neutrons rapides au sodium, les aciers renforcés par dispersion d’oxydes (ODS) sont envisagés pour leur excellente résistance à l’irradiation et leur tenue mécanique à haute température. Néanmoins, des difficultés sont rencontrées quant à la maitrise de leur élaboration et de leur mise en forme, ainsi que sur la prédiction de leur comportement en fluage. Les travaux présentés visent à améliorer la compréhension des mécanismes de fluage d’aciers ferritiques renforcés par dispersion et à étudier les voies d’amélioration possible.Dans un premier temps, le fluage d’aciers ferritiques renforcés par dispersion obtenus par cobroyage et extrusion à été étudié grâce à deux aciers ODS à 14pd.% Cr et 18pd.%Cr, ainsi qu’un acier 18pd.%Cr renforcé par dispersion de nitrures (NDS). Une caractérisation mécanique et microstructurale (SEM – EBSD – EDX et STEM) d’éprouvettes sollicitées en fluage à respectivement 650°C et 800°C est réalisée les aciers ODS Fe18Cr et Fe14Cr. La faible déformation et la rupture brutale classiquement observée sur ce type d’acier est mise en évidence. La diminution continue de leur vitesse de déformation et l’absence d’évolutions microstructurales indiquent que le fluage se produit essentiellement dans le stade primaire. L’acier ferritique NDS a ensuite été étudié. Un phénomène de déformation superplastique (plus de 110%) a été mis en évidence à 650°C en traction entre 10-3 s-1 et 10-2 s-1, ainsi qu’une recristallisation dynamique continue au dessus de 10-2 s-1. En fluage à 650°C, l’acier NDS présente une faible déformation (moins de 1%) et une rupture brutale : il s’agit donc d’un comportement générique des aciers ferritiques renforcés par dispersion, indépendamment du type de précipité. La déformation se produisant lors du stade primaire du fluage, le comportement de ces aciers ODS et NDS a été modélisé en se basant sur l’approche de Kocks et Mecking, fondée sur l’activation thermique du glissement après franchissement des précipités par montée ou glissement dévié. Ce modèle fournit une origine physique à la contrainte seuil observée lors du fluage des aciers ODS. La déformation en fluage des deux ODS et de l’acier NDS a été simulée à partir de coefficients déterminés expérimentalement et de paramètres optimisés. Les lois de Norton, les densités de dislocation et les limites élastiques simulées sont cohérentes avec les valeurs obtenues par les essais de fluage, de traction et des mesures (STEM – EFTEM) de la densité de dislocations. Une investigation des causes de rupture brutale en fluage a ensuite été menée sur l’ODS 14pd.%Cr : grâce à un essai de fluage interrompu à 800°C alterné avec des recuits à 1050°C, la rupture brutale a été retardée et une déformation de 1.5% a été atteinte. Un suivi de l’endommagement par tomographie X et un essai de fluage après vieillissement semblent éliminer l’endommagement macroscopique et la phase σ comme cause de la rupture brutale. Un scénario basé sur une déformation critique a été proposé. Pour finir, les difficultés liées à la mise en forme des ODS ferritiques ont conduit à concevoir une nouvelle nuance ODS martensitique à 11pd.% Cr et à évaluer un nouveau procédé d’atomisation de poudres (GARS). Il apparait que la compaction directe après atomisation par la voie alternative n’améliore pas les performances de ces aciers. En revanche, après broyage, la nouvelle composition présente un potentiel intéressant en traction et en fluage à 650°C. / Within the French research program for Sodium Fast Reactor (SFR) core material, oxide dispersion strengthened (ODS) steels are considered for their resistance to irradiation swelling and their good creep properties at high temperature. Their elaboration, their processing and their creep mechanism still represent challenges for material science. The aim of this work is to improve the understanding of the creep mechanisms and to investigate new fabrication route to improve these materials.First, the creep of dispersion strengthened ferritic steels produced by mechanical alloying and extrusion is studied, based on two ODS steels with 14wt.%Cr and 18wt.%Cr, and a nitride dispersion strengthened (NDS) steel with 18wt.%Cr. A microstructural (SEM-EBSD-STEM) characterization has been carried out on the two ferritic ODS steels loaded at 650°C and 800°C: a low creep strain (<0.5%) and a brutal fracture are observed. The continuous decrease of the creep rate without any microstructural change indicates a late primary stage. Then the tensile and creep behaviors of the NDS ferritic steel have been studied: a superplastic deformation, up to 110%, has been evidenced at 650°C between 10-3 s-1 and 10-2 s-1, as well as a continuous dynamic recrystallization at strain rate higher than 10-2 s-1. However, during creep tests at 650°C, the NDS steel presents the same characteristics as the ODS steels: low creep strain and brutal fracture. This behavior seems to be generic for dispersion strengthened ferritic steels obtained by mechanical alloying, regardless the type of precipitate. As the deformation occurs during the primary stage, a Kocks and Mecking model has been developed based on the thermal activation of the dislocation glide after crossing the precipitate by climb or cross-slip. This model provides a physical explanation for the threshold stress observed during the creep of ODS steels. The creep strain of the two ODS steels and the NDS steel has been simulated with experimentally determined coefficients and fitted parameters. The simulated Norton laws, dislocation density and yield stress are consistent with experimental data obtained respectively by the creep tests, by dislocation density determination (STEM-EFTEM) and tensile tests. An investigation of the creep fracture mechanisms has been performed. The creep fracture was delayed using high temperature heat treatments at 1050°C between interrupted creep tests at 800°C on the Fe14Cr ODS steel and a total elongation of 1.5% has been reached by this means. By analyzing X-ray tomography and creep test after ageing treatment, it appears that the macroscopic elongated cavities and sigma phase are not likely to explain the brutal fracture, therefore a scenario based on a critical deformation is proposed. Finally, the processing difficulties of the ferritic ODS steel lead to the design of a new martensitic 11wt. % Cr ODS steel and the evaluation of a new atomization process (GARS). This new atomization process did not improve the mechanical properties of these steels. However, after milling, encouraging results are observed since the first mechanical and microstructural characterizations displayed good tensile and creep properties.